X-ray diffraction and infrared reflection spectroscopy data have confirmed the electrosynthesis of copper dicyanamide films by cyclic voltammetry and potentiostatic electrolysis. An insoluble Cu(I)dca film can be synthesized on a gold or copper electrode by the reduction of Cu(II) or oxidation of Cu(0) in aqueous or methanolic solutions containing dicyanamide ions. By resorting to the use of the ruthenium hexaammine redox probe the Cu(I)dca film was shown to be electronically conductive although the deposition rate decreases when the film formation proceeds.Depending on the applied potential, not only Cu(I)dca but also Cu(II)dca can be formed by oxidation of a copper electrode in presence of dicyanamide ions dissolved in methanol. The powder obtained by electrolysis at 1 V vs Hg/Hg2SO4 made essentially of Cu(II)dca presents a specific surface area of (183 ± 59) m2/g. This material can adsorb preferentially methyl orange and Congo red dyes compared to methylene blue whereas no marked difference is obtained between CO and CO2 adsorption.
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